A kind of preparation method of high-purity fluoroethylene carbonate

A technology of pure fluoroethylene carbonate and chloroethylene carbonate, which is applied in the field of preparation of high-purity fluoroethylene carbonate, can solve the problems of low product purity and high equipment requirements, achieve high purity, reduce impurity content, improve The effect of purity

Active Publication Date: 2019-10-11
DO FLUORIDE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a method for preparing high-purity fluoroethylene carbonate, thereby solving the problems of low purity of the product obtained in the existing method and high requirements for equipment in the purification process

Method used

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  • A kind of preparation method of high-purity fluoroethylene carbonate
  • A kind of preparation method of high-purity fluoroethylene carbonate
  • A kind of preparation method of high-purity fluoroethylene carbonate

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Embodiment 1

[0030] The preparation method of the high-purity fluoroethylene carbonate of the present embodiment, technological process is as follows figure 1 shown, including the following steps:

[0031] 1) 1 kg of chloroethylene carbonate raw material and anhydrous hydrogen fluoride liquid are passed into the microchannel reactor at the same time in a molar ratio of 1:1 for reaction, the reaction temperature is -15°C, and the reaction time is 7 minutes;

[0032] 2) Step 1) After the reaction is complete, transfer the reaction liquid and reaction gas to the tank reactor, and pass dry high-purity nitrogen gas to replace the hydrogen chloride gas in the tank reactor. The temperature in the reactor is controlled at -15°C, and the nitrogen gas The time is 3min;

[0033] 3) Step 2) After the replacement is complete, feed a fluorine-nitrogen mixed gas with a fluorine-containing gas volume content of 5% and react with unreacted chloroethylene carbonate. In the fluorine-nitrogen mixed gas, fluo...

Embodiment 2

[0041] The preparation method of the high-purity fluoroethylene carbonate of the present embodiment may further comprise the steps:

[0042] 1) Feed 1 kg of chloroethylene carbonate raw material and anhydrous hydrogen fluoride liquid into a microchannel crystallizer at the same time in a molar ratio of 1:1.1 for reaction, the reaction temperature is 0°C, and the reaction time is 10 minutes;

[0043] 2) Step 1) After the reaction is complete, transfer the reaction liquid and reaction gas to the tank reactor, and pass dry high-purity nitrogen gas to replace the hydrogen chloride gas in the tank reactor. The temperature in the reactor is controlled at 0°C, and the nitrogen gas The time is 10 minutes;

[0044] 3) Step 2) After the replacement is complete, feed a fluorine-nitrogen mixed gas with a fluorine-containing gas volume content of 5% and react with unreacted chloroethylene carbonate. In the fluorine-nitrogen mixed gas, fluorine and chloroethylene carbonate The molar ratio ...

Embodiment 3

[0052] The preparation method of the high-purity fluoroethylene carbonate of the present embodiment may further comprise the steps:

[0053] 1) Feed 1 kg of chloroethylene carbonate raw material and anhydrous hydrogen fluoride liquid into a microchannel crystallizer at the same time in a molar ratio of 1:1.15 for reaction, the reaction temperature is 16°C, and the reaction time is 25 minutes;

[0054] 2) Step 1) After the reaction is complete, transfer the reaction liquid and reaction gas to the tank reactor, and pass dry high-purity nitrogen gas to replace the hydrogen chloride gas in the tank reactor. The temperature in the reactor is controlled at 18°C, and the nitrogen gas The time is 10 minutes;

[0055] 3) Step 2) After the replacement is complete, feed a fluorine-nitrogen mixed gas with a fluorine-containing gas volume content of 10% and react with unreacted chloroethylene carbonate. In the fluorine-nitrogen mixed gas, fluorine and chloroethylene carbonate The molar ra...

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Abstract

The invention relates to a preparation method of high-purity fluoroethylene carbonate. The preparation method comprises the following steps: 1) reacting chloroethylene carbonate raw materials with hydrogen fluoride liquid to obtain a mixture; 2) adding metal oxides to the mixture for deacidification reaction, and filtering to obtain a filtrate; 3) adding Solvents are mixed, and the temperature is lowered to crystallize to obtain fluoroethylene carbonate crystals, and water is removed to obtain high-purity fluoroethylene carbonate. The preparation method of high-purity fluoroethylene carbonate of the present invention uses chloroethylene carbonate and anhydrous hydrogen fluoride liquid as raw materials to carry out liquid-liquid reaction, and prepares high-purity fluoroethylene carbonate through the processes of acid removal reaction, temperature-lowering crystallization, and temperature-raising water removal process , the purity of the obtained product is more than 99.5%. The preparation method has simple process control, less side reactions, easy purification, high purity of the reaction product, low cost, and is convenient for industrialized production.

Description

technical field [0001] The invention belongs to the field of synthesis of fluoroethylene carbonate, in particular to a preparation method of high-purity fluoroethylene carbonate. Background technique [0002] With the improvement of people's living standards and the gradual depletion of fossil energy, the development of new energy has gradually been mentioned by governments at the strategic level. However, the current constraints on the development of new energy vehicles are mainly mileage, cost and safety. Depending on the various materials used in the manufacture of new energy vehicles, the safety mainly depends on the lithium-ion battery of the power supply device, and the electrolyte determines the safety of the lithium-ion battery. At present, the development of new energy vehicles has higher and higher requirements on the performance of the electrolyte. [0003] Fluoroethylene carbonate (FEC), as an additive to the electrolyte of lithium-ion batteries, can inhibit the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/42
CPCC07D317/42
Inventor 侯红军薛旭金于贺华刘海霞司腾飞杨明霞薛峰峰罗传军李云峰刘海庆于洋张照坡
Owner DO FLUORIDE CHEM CO LTD
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